Dimethylformamide → HCID 86042697, 화합물

HRID 1698395노트

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HRID 1698395 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([N:8]([CH2:11][CH3:12])[CH2:9][CH3:10])=[C:4]([C:13]([CH3:16])([CH3:15])[CH3:14])[CH:3]=1.[Li]CCCC.CN([CH:25]=[O:26])C.[Cl-].[NH4+]>C1COCC1>[C:13]([C:4]1[CH:3]=[C:2]([CH:7]=[CH:6][C:5]=1[N:8]([CH2:11][CH3:12])[CH2:9][CH3:10])[CH:25]=[O:26])([CH3:16])([CH3:15])[CH3:14]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 25517Ammonium ChlorideHCID 66671963(4-Bromo-2-tert-butylphenyl)diethylamineHCID 178418339Butyllithium

생성물 1

HCID 86042697HCID 86042697, 화합물수율 102.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
-78 °C

실험 절차

3.6 g (13 mmol) of (4-bromo-2-tert-butylphenyl)-diethylamine are diluted in 100 ml of THF, under a stream of nitrogen. The medium is cooled to −78° C. and then 7.8 ml (20 mmol) of a 2.5M solution of nBuLi are added. After stirring for 45 minutes, 1.5 ml (20 mmol) of DMF are added and the solution is brought back to ambient temperature. After 15 minutes, the mixture is poured into a saturated solution of ammonium chloride and then extracted twice with ethyl acetate. The organic phase is dried over sodium sulphate and then concentrated to dryness. 3.1 g of 3-tert-butyl-4-diethylaminobenzaldehyde are obtained in the form of a yellow oil (yield=100%).

후처리

  1. customis brought back to ambient temperature
  2. waitAfter 15 minutes
  3. extractionextracted twice with ethyl acetate
  4. dry with materialThe organic phase is dried over sodium sulphate
  5. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-fb66f79ea88d45e2a2f2498efbdd22a7
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08163952B2

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